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- Title
Determination of Aminoalcohols as Silyl Derivatives with Three Derivatizing Agents by Gas Chromatography with Mass Spectrometry Detection.
- Authors
Novikova, I. V.; Novikov, R. I.; Smirnova, Zh. V.; Aleksenko, S. S.; Kondrat'ev, V. B.
- Abstract
Approaches are developed to the separation and identification of eleven β-amino alcohols, markers of nitrogen-containing toxic chemicals (V-gases, nitrogen mustards and BZ), as trimethyl-(TMS) and tert-butyldiphenylsilyl derivatives by gas chromatography with mass spectrometry detection. The conditions for the joint silylation of β-amino alcohols with reagents 1,1,1,3,3,3-hexamethyldisilazane (HMDS), N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), and tert-butyldiphenylchlorosilane (TBDPS) are optimized. The TBDPS reagent for the derivatization of β-amino alcohols is proposed for the first time. It is shown that the optimum temperature for ensuring the derivatization of a mixture of all β-amino alcohols with HMDS is 40°C and reaction time is 15 min; with BSTFA, 60°C and 30 min; and with TBDPS, 80°C and 45 min. At that, in the case of HMDS, it is necessary to introduce an activating additive of 0.02% iodine, and for TBDPS, N-methylimidazole in a ratio of 1 : 2. The reactivity of β-amino alcohols with respect to silylating agents decreases in the series of N,N-dialkylaminoethanols: N-alkyldiethanolamines—triethanolamine—3‑quinuclidinol. The structural isomers of methylpropyl- and methylisopropylethanolamine can be separated only as TBDPS-derivatives on a stationary phase of medium polarity (VF-1701 MS). The limits of detection for β-aminoalcohols as TMS derivatives lie in the range of 0.05–0.5 μg/mL, and for TBDPS derivatives, 0.2–0.8 μg/mL. The results obtained ensure the reliable identification of β-amino alcohols in a mixture at concentrations of >1 μg/mL.
- Subjects
MASS spectrometry; GAS chromatography; STRUCTURAL isomers; POISONS; NITROGEN mustards; CHIRAL stationary phases
- Publication
Journal of Analytical Chemistry, 2022, Vol 77, Issue 12, p1561
- ISSN
1061-9348
- Publication type
Article
- DOI
10.1134/S1061934822120115